Dichloromethane → 3-[(2-Chloroethyl)amino]thiolane-1,1-dione

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

A mixture of 3-((2-hydroxyethyl)amino)tetrahydrothiophene 1,1-dioxide (260 mg, 1.451 mmol) and sulfurous dichloride (863 mg, 7.25 mmol) in dichloroethane (3 mL) was heated up at 78° C. for 3 hours. The mixture was cooled to room temperature and concentrated under reduced pressure to provide the black oil. To this black oil was added THF (5 mL) and dichloromethane (5 mL), grey-white solid was observed. The solid was filtered and collected to provide the desired product as a grey solid (230 mg, 80%). LCMS: m/e 198.1 (M+H)+, 0.60 min (method 6).

Herkunft & Nachweise